CN105842725B - The assay method of the specific activity of tritiated water vapour in a kind of air - Google Patents
The assay method of the specific activity of tritiated water vapour in a kind of air Download PDFInfo
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- CN105842725B CN105842725B CN201610172939.5A CN201610172939A CN105842725B CN 105842725 B CN105842725 B CN 105842725B CN 201610172939 A CN201610172939 A CN 201610172939A CN 105842725 B CN105842725 B CN 105842725B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/17—Circuit arrangements not adapted to a particular type of detector
- G01T1/178—Circuit arrangements not adapted to a particular type of detector for measuring specific activity in the presence of other radioactive substances, e.g. natural, in the air or in liquids such as rain water
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Abstract
The invention discloses a kind of assay methods of the specific activity of tritiated vapor in air, it specifically includes using the tritiated vapor in 3A molecular sieves absorption air, the tritiated water in 3A molecular sieves after water suction is in freeze drying plant through freezing, it is collected after distillation, tritiated water after collection cleans after ion exchange resin absorption and micro-filtration is detected the specific activity of tritiated water, the method of the present invention is higher due to the collecting efficiency to tritiated water, the residual of sampling media is few, it tritiated water can thus be collected in air, and the specific activity of tritiated water can be detected when specific activity is smaller, the accuracy of data is higher；Method collecting efficiency using the present invention can reach 99%, sampling media residual quantity ＜ 1%.
Description
Technical field
The present invention relates to the activity measurement method of radgas, the ratio of tritiated water vapour is lived in specifically a kind of air
The assay method of degree.
Background technology
Important radioactive gas nuclide of the tritium as fission power operation heap discharge, various nuclear facilities are released into ambient enviroment
Tritium can lead to the raising of ambient atmosphere tritium activity, and be operated in nuclear power plant reactor workshop and the work in relation to auxiliary plant
Tritium can be taken in by all means by making personnel, to cause a degree of interior irradiation, therefore, improve the tritium activity in air
Accuracy of detection is the critical issue that gaseous state tritium measures.
Tritium activity method for measuring at present includes mainly direct method and indirect method, and direct method is to use detection of gas
Device such as ionisation chamber, proportional counter carry out the measurement of gas, and indirect method is to be catalytically oxidized to tritium to utilize sudden strain of a muscle after tritiated water
Bright bulk detector measures, the former sensitivity is low, and when the specific activity of tritium is relatively low, instrument inspection does not measure accurate numerical value,
It is not suitable for the detection of tritium in regular air, may be only available for Tritium measurement in radiation work place, although the latter's sensitivity
It is higher, it is simple, can handle a large amount of samples, but the existing method of sampling cannot achieve it is accurate under northern low temperature environment in winter
Sampling.
Invention content
To solve the above problems, the object of the present invention is to provide a kind of measurement sides of the specific activity of tritiated water vapour in air
Method.
The present invention to achieve the above object, is achieved through the following technical solutions：
The assay method of the specific activity of tritiated water vapour, includes the following steps in a kind of air：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
After activation is housed in receipts bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition, the absorption bottle A and absorption bottle B
The required device of acquisition of sample is mounted on the position of 0.9~1.1m high of ground, starts air by 3A molecular sieves
Pump, adjusting flow control valve makes the flow of flowmeter be located at 0.5~5.0L/min, starts to sample, when discoloration silica gel indicates pipe
Silica gel closes air pump, flow control valve successively after becoming pink from blue, record integrated flux, remove absorption bottle A and suction
Receive will acquire after bottle B the molecular sieve after tritiated water pour out it is spare；Microfiltration membrane is housed in the particle filter；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump and collect tritiated water 48~50 hours
Obtain tritiated water；
3. by step, 2. ion exchange resin is added in gained tritiated water, stirs to the conductivity of tritiated water and is down to 5 μ S/cm,
Then tritiated water to be measured is obtained with aqueous micro-filtrate membrane filtration, the mass ratio of the tritiated water and ion exchange resin is 4~5:1；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water.
Preferably, the filter membrane being equipped in the particle filter is PTFE micron order hydrophylic filter membranes.
Preferably, the ion exchange resin is EC20MB electron level mixture iron exchange resins.
The assay method of the specific activity of tritiated water vapour, includes the following steps in further preferred air：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
After activation is housed in receipts bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition, the absorption bottle A and absorption bottle B
The required device of acquisition of sample is mounted on the position of ground 1m high, starts air pump, adjust stream by 3A molecular sieves
Adjustable valve makes the flow of flowmeter be located at 1.0L/min, starts to sample, when discoloration silica gel indicates that the silica gel of pipe is become from blue
Air pump, flow control valve are closed after pink successively, integrated flux is recorded, tritium will be acquired after removing absorption bottle A and absorption bottle B
Molecular sieve after change water is poured out spare；The filter membrane being equipped in the particle filter is PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump collection tritiated water and obtain for 48 hours
Tritiated water；
3. by step, 2. EC20MB electron level mixture iron exchange resins are added in gained tritiated water, stir to the electricity of tritiated water
Conductance is down to 5 μ S/cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration, and the tritiated water is mixed with EC20MB electron levels
The mass ratio for closing ion exchange resin is 4:1；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water.
The present invention has the following advantages compared with prior art：
Using the tritiated water vapour in 3A molecular sieves absorption air, the tritiated water in 3A molecular sieves after water suction exists the present invention
It is collected after freezing, distilling in freeze drying plant, the tritiated water after collection is adsorbed through ion exchange resin and micro-filtration
Removal of impurities is detected the specific activity of tritiated water afterwards, and method of the invention is since the collecting efficiency to tritiated water is higher, sampling media
Residual it is few, thus tritiated water can be collected in air, and the ratio of tritiated water can be detected when specific activity is smaller
The accuracy of activity, data is higher；Equipment investment used in the method for the present invention is few, and connection is simple to operation, to environmental requirement
It is low, can also detection be collected to the tritiated water in air, be particularly suitable for northern China winter low temperature ring under general environment
It is difficult to collect sample using other methods under border or instrument precision is relatively low to be carried out to the low-activity tritiated water in air
When accurate measurement；The method design of the present invention is exquisite, and before 3A molecular sieves adsorb the tritiated water in air, air first passes through grain
The filtering of sub- filter removes the dust particles in air, can improve the efficiency of 3A molecular sieves absorption tritiated water, and utilizes 3A
Molecular sieve only adsorbs the molecule that vapor does not adsorb the biggers such as carbon dioxide, amino molecule, and vapor and other molecules are separated, from
And improve the precision of sampling；Post-processing is using other impurities in ion exchange resin absorption tritiated water, so that tritiated water is lived
Its numerical value is detected when spending relatively low；Method collecting efficiency using the present invention can reach 99%, sampling media residual quantity ＜
1%.
Description of the drawings
Fig. 1 is tritiated water sampling apparatus schematic diagram in air；
Reference numeral：1 particle filter, 2 flow control valves, 3 flowmeters, 4 absorption bottle A, 5 absorption bottle B, 6 air pumps, 7
Change colour silica gel instruction pipe.
Specific implementation mode
The object of the present invention is to provide a kind of assay methods of the specific activity of tritiated water vapour in air, pass through following technology
Scheme is realized：
The assay method of the specific activity of tritiated water vapour, includes the following steps in a kind of air：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
After activation is housed in receipts bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition, the absorption bottle A and absorption bottle B
The required device of acquisition of sample is mounted on the position of 0.9~1.1m high of ground, starts air by 3A molecular sieves
Pump, adjusting flow control valve makes the flow of flowmeter be located at 0.5~5.0L/min, starts to sample, when discoloration silica gel indicates pipe
Silica gel closes air pump, flow control valve successively after becoming pink from blue, record integrated flux, remove absorption bottle A and suction
Receive will acquire after bottle B the molecular sieve after tritiated water pour out it is spare；Microfiltration membrane is housed in the particle filter；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump and collect tritiated water 48~50 hours
Obtain tritiated water；
3. by step, 2. ion exchange resin is added in gained tritiated water, stirs to the conductivity of tritiated water and is down to 5 μ S/cm,
Then tritiated water to be measured is obtained with aqueous micro-filtrate membrane filtration, the mass ratio of the tritiated water and ion exchange resin is 4~5:1；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water.
Preferably, the filter membrane being equipped in the particle filter is PTFE micron order hydrophylic filter membranes.
Preferably, the ion exchange resin is EC20MB electron level mixture iron exchange resins.
The assay method of the specific activity of tritiated water vapour, includes the following steps in further preferred air：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
After activation is housed in receipts bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition, the absorption bottle A and absorption bottle B
The required device of acquisition of sample is mounted on the position of ground 1m high, starts air pump, adjust stream by 3A molecular sieves
Adjustable valve makes the flow of flowmeter be located at 1.0L/min, starts to sample, when discoloration silica gel indicates that the silica gel of pipe is become from blue
Air pump, flow control valve are closed after pink successively, integrated flux is recorded, tritium will be acquired after removing absorption bottle A and absorption bottle B
Molecular sieve after change water is poured out spare；The filter membrane being equipped in the particle filter is PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump collection tritiated water and obtain for 48 hours
Tritiated water；
3. by step, 2. EC20MB electron level mixture iron exchange resins are added in gained tritiated water, stir to the electricity of tritiated water
Conductance is down to 5 μ S/cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration, and the tritiated water is mixed with EC20MB electron levels
The mass ratio for closing ion exchange resin is 4:1；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water.
Below in conjunction with specific embodiment, the invention will be further described.
Korea has carried out the 4th nuclear test at the beginning of 2016, and China is to respond Korea's nuclear test, to the ground of border area four
The radiation of point has carried out emergent test, i.e., to the tritiated water in the gas of border overhead collect and detect, specific steps respectively
And data processed result is as follows：
Embodiment 1
To the assay method of the specific activity of tritiated water vapour in the air of place 1 (test temperature is about 278K), including with
Lower step：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
Bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition are received, as shown in Figure 1, being filled in the absorption bottle A and absorption bottle B
There are the 3A molecular sieves after activation, the volume of 3A molecular sieves accounts for 2/3rds or more of absorption bottle A and absorption bottle B, by sample collection
Required device is mounted on the position of ground 1.0m high, starts air pump, and adjusting flow control valve makes flowmeter
Flow is located at 2.0L/min, starts to sample, and is closed successively after the silica gel that changes colour indicates that the silica gel of pipe becomes pink from blue empty
Air pump, flow control valve, record cumulative flow magnitude are 6.135m3, removing after absorption bottle A and absorption bottle B will be after acquisition tritiated water
Molecular sieve pour out it is spare；Microfiltration membrane is housed in the particle filter；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump and collect tritiated water 48~50 hours
Obtain 10.44 grams of tritiated water；
3. by step, 2. 2.00 grams of ion exchange resin is added in gained tritiated water, stirs to the conductivity of tritiated water and is down to 5 μ
Then S/cm obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water；The specific method is as follows：Pipette waiting for for m=8.0g
Liquid sample is surveyed to polytetrafluoroethylene (PTFE) counting vial, adds III scintillation solutions of 12.0mL Hisafe, concussion seals after mixing, uses
The wet cotton balls of alcohol wipes sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, is protected from light 2 hours
After measure 1000min.Test specimens are taken out from Low background liquid scintillation energy disperse spectroscopy and the tritium that 0.1g activity is 8.72Bq/g is added
Standard solution, concussion are uniformly mixed, and use Low background liquid scintillation energy disperse spectroscopy to test 1000min again after wiping, being protected from light.Record mark
Quasi- sample counting rate is 12.528cpm, and sample to be tested counting rate is 0.961cpm, this bottom sample counting rate is 0.872cpm.
Embodiment 2
To the assay method of the specific activity of tritiated water vapour in the air of place 2 (test temperature is about 273K), including with
Lower step：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
Bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition are received, as shown in Figure 1, being filled in the absorption bottle A and absorption bottle B
There are the 3A molecular sieves after activation, the volume of 3A molecular sieves accounts for 2/3rds or more of absorption bottle A and absorption bottle B, by sample collection
Required device is mounted on the position of ground 1.0m high, starts air pump, and adjusting flow control valve makes flowmeter
Flow is located at 2.0L/min, starts to sample, and is closed successively after the silica gel that changes colour indicates that the silica gel of pipe becomes pink from blue empty
Air pump, flow control valve, record cumulative flow magnitude are 6.135m3, removing after absorption bottle A and absorption bottle B will be after acquisition tritiated water
Molecular sieve pour out it is spare；The filter membrane being equipped in the particle filter is PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump collection tritiated water and obtain for 48 hours
9.49 grams of tritiated water；
3. by step, 2. 2.10 grams of EC20MB electron levels mixture iron exchange resin is added in gained tritiated water, stirs to tritiated
The conductivity of water is down to 5 μ S/cm, then obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water；The specific method is as follows：Pipette waiting for for m=8.0g
Liquid sample is surveyed to polytetrafluoroethylene (PTFE) counting vial, adds III scintillation solutions of 12.0mL Hisafe, concussion seals after mixing, uses
The wet cotton balls of alcohol wipes sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, and it is small to be protected from light 2.5
When after measure 1000min.It is 8.72Bq/g's to take out test specimens from Low background liquid scintillation energy disperse spectroscopy and 0.1g activity is added
Tritium standard solution, concussion are uniformly mixed, and use Low background liquid scintillation energy disperse spectroscopy to test 1000min again after wiping, being protected from light.Record
Standard sample counting rate is 13.008cpm, and sample to be tested counting rate is 1.008cpm, this bottom sample counting rate is 0.872cpm.
Embodiment 3
To the assay method of the specific activity of tritiated water vapour in the air in place 3 (test temperature 263K), including it is following
Step：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
Bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition are received, as shown in Figure 1, being filled in the absorption bottle A and absorption bottle B
There are the 3A molecular sieves after activation, the volume of 3A molecular sieves accounts for 2/3rds or more of absorption bottle A and absorption bottle B, by sample collection
Required device is mounted on the position of ground 0.9m high, starts air pump, and adjusting flow control valve makes flowmeter
Flow is located at 3.0L/min, starts to sample, and is closed successively after the silica gel that changes colour indicates that the silica gel of pipe becomes pink from blue empty
Air pump, flow control valve, record cumulative flow magnitude are 10.214m3, removing after absorption bottle A and absorption bottle B will be after acquisition tritiated water
Molecular sieve pour out it is spare；Microfiltration membrane is housed in the particle filter；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump and collect tritiated water 48~50 hours
Obtain 8.85 grams of tritiated water；
3. by step, 2. 2.09 grams of ion exchange resin is added in gained tritiated water, stirs to the conductivity of tritiated water and is down to 5 μ
Then S/cm obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water；The specific method is as follows：Pipette waiting for for m=8.0g
Liquid sample is surveyed to polytetrafluoroethylene (PTFE) counting vial, adds III scintillation solutions of 12.0mL Hisafe, concussion seals after mixing, uses
The wet cotton balls of alcohol wipes sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, is protected from light 3 hours
After measure 1000min.Test specimens are taken out from Low background liquid scintillation energy disperse spectroscopy and the tritium that 0.1g activity is 8.72Bq/g is added
Standard solution, concussion are uniformly mixed, and use Low background liquid scintillation energy disperse spectroscopy to test 1000min again after wiping, being protected from light.Record mark
Quasi- sample counting rate is 14.024cpm, and sample to be tested counting rate is 1.012cpm, this bottom sample counting rate is 0.872cpm.
Embodiment 4
To the assay method of the specific activity of tritiated water vapour in the air in place 4 (test temperature 258K), including it is following
Step：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, suction
Bottle A, absorption bottle B, discoloration silica gel instruction pipe and air pump composition are received, as shown in Figure 1, being filled in the absorption bottle A and absorption bottle B
There are the 3A molecular sieves after activation, the volume of 3A molecular sieves accounts for 2/3rds or more of absorption bottle A and absorption bottle B, by sample collection
Required device is mounted on the position of ground 0.9m high, starts air pump, and adjusting flow control valve makes flowmeter
Flow is located at 3L/min, starts to sample, and air is closed successively after the silica gel that changes colour indicates that the silica gel of pipe becomes pink from blue
Pump, flow control valve, record cumulative flow magnitude are 12.245m3, removing after absorption bottle A and absorption bottle B will be after acquisition tritiated water
Molecular sieve is poured out spare；Microfiltration membrane is housed in the particle filter；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, freezed
To -20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump collection tritiated water and obtain for 50 hours
9.68 grams of tritiated water；
3. by step, 2. 1.80 grams of ion exchange resin is added in gained tritiated water, stirs to the conductivity of tritiated water and is down to 5 μ
Then S/cm obtains tritiated water to be measured with aqueous micro-filtrate membrane filtration；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, root
The specific activity of tritiated water vapour in air is calculated according to the activity meter of tritium in tritiated water；The specific method is as follows：Pipette waiting for for m=8.0g
Liquid sample is surveyed to polytetrafluoroethylene (PTFE) counting vial, adds III scintillation solutions of 12.0mL Hisafe, concussion seals after mixing, uses
The wet cotton balls of alcohol wipes sample to be tested counting vial outer wall, and counting vial is put into Low background liquid scintillation energy disperse spectroscopy, is protected from light 3 hours
After measure 1000min.Test specimens are taken out from Low background liquid scintillation energy disperse spectroscopy and the tritium that 0.1g activity is 8.72Bq/g is added
Standard solution, concussion are uniformly mixed, and use Low background liquid scintillation energy disperse spectroscopy to test 1000min again after wiping, being protected from light.Record mark
Quasi- sample counting rate is 13.254cpm, and sample to be tested counting rate is 0.989cpm, this bottom sample counting rate is 0.872cpm.
Comparative example
The vapor in 2 air of place is acquired using tritium sampler in MARC7000 type air, then water is steamed
The activity of tritium in gas is detected, and does not detect that the vapor in 2 air of place contains tritiated water.
Result treatment
The data of Examples 1 to 4 are handled according to following formula, obtain tritiated water vapour in each place air
The data of specific activity are as shown in table 1.
1. instrument efficiency calculation formula：
In formula, E --- instrument efficiency, %；
N2--- standard sample counting rate, cpm；
N1--- --- sample to be tested counting rate, cpm；
A1--- tritium standard solution activity, Bq/g；
m1--- tritium standard solution quality, g is added.
2. tritiated water sample activity concentration calculation formula：
In formula, A2--- tritiated water sample activity, Bq/g；
N1--- sample to be tested counting rate, cpm；
N0--- --- background sample counting rate, cpm；
E --- instrument efficiency, %；
M --- tritiated water volume of sample, g.
3. cumulative sample volume is modified to mark condition volume calculation formula：
In formula, V --- acquisition air mark condition volume, m3；
V0--- acquisition sample cumulative volume, m3；
P0--- atmospheric pressure when sample collection, Pa；
Atmospheric pressure under P --- standard state, 101.3kPa；
Temperature under T --- standard state, K；
T0--- temperature when sample collection, K.
4. tritium raito (T.R) Activity Calculation formula in air：
In formula, A --- tritiated water steam specific activity, Bq/m in air3；
A2--- tritiated water sample activity, Bq/mL；
M --- tritiated water volume of sample, mL；
V --- acquisition volume of air (mark condition), m3；
m1--- acquisition tritiated water population of samples product, mL.
The specific activity result table of tritiated water vapour in the air of 1 Examples 1 to 4 of table
Show that tritium sampler cannot achieve in the dense of tritium in existing air by the data comparison of embodiment 2 and comparative example
Accurate sampling when spending relatively low, thus cannot accurately detect the specific activity of the tritiated vapor in air, sampling of the invention
Method can realize the accurate sampling to tritiated water in air at low ambient temperatures, when especially tritiated water concentration is relatively low in air
Realize the accurate measurements to radiation environment.
Claims (2)
1. the assay method of the specific activity of tritiated water vapour in a kind of air, it is characterised in that：Include the following steps：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, absorption bottle
A, equipped with 3A points after activation in absorption bottle B, discoloration silica gel instruction pipe and air pump composition, the absorption bottle A and absorption bottle B
The required device of acquisition of sample is mounted on the position of 0.9~1.1m high of ground, starts air pump, adjust by son sieve
Throttling adjustable valve so that the flow of flowmeter is located at 0.5~5.0L/min, start to sample, when discoloration silica gel instruction pipe silica gel by
Blue closes air pump, flow control valve successively after becoming pink, integrated flux is recorded, after removing absorption bottle A and absorption bottle B
Molecular sieve after acquisition tritiated water is poured out spare；PTFE micron order hydrophylic filter membranes are housed in the particle filter；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, be refrigerated to-
20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump collection tritiated water and obtain for 48~50 hours
To tritiated water；
3. by step, 2. ion exchange resin is added in gained tritiated water, stirs to the conductivity of tritiated water and is down to 5 μ S/cm, then
Tritiated water to be measured is obtained with aqueous micro-filtrate membrane filtration, and the mass ratio of the tritiated water and ion exchange resin is 4~5:1；It is described
Ion exchange resin be EC20MB electron level mixture iron exchange resins；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, according to tritium
The activity meter for changing tritium in water calculates the specific activity of tritiated water vapour in air.
2. the assay method of the specific activity of tritiated water vapour in a kind of air according to claim 1, it is characterised in that：Packet
Include following steps：
1. the acquisition of sample：The required device of acquisition of sample is by particle filter, flow control valve, flowmeter, absorption bottle
A, equipped with 3A points after activation in absorption bottle B, discoloration silica gel instruction pipe and air pump composition, the absorption bottle A and absorption bottle B
The required device of acquisition of sample is mounted on the position of ground 1m high, starts air pump, adjust flow tune by son sieve
Section valve makes the flow of flowmeter be located at 1.0L/min, starts to sample, when discoloration silica gel indicates that the silica gel of pipe becomes pink from blue
Air pump, flow control valve are closed after color successively, integrated flux is recorded, tritiated water will be acquired after removing absorption bottle A and absorption bottle B
Molecular sieve afterwards is poured out spare；The filter membrane being equipped in the particle filter is PTFE micron order hydrophylic filter membranes；
2. the molecular sieve after step 1. gained acquisition tritiated water is fitted into the sample disc of vacuum refrigeration device, be refrigerated to-
20 DEG C, then sample disc is put on the specimen holder of vacuum refrigeration device, starts vacuum pump collection tritiated water and obtain tritium in 48 hours
Change water；
3. by step, 2. EC20MB electron level mixture iron exchange resins are added in gained tritiated water, stir to the conductivity of tritiated water
Be down to 5 μ S/cm, then obtain tritiated water to be measured with aqueous micro-filtrate membrane filtration, the tritiated water mixed with EC20MB electron levels from
The mass ratio of sub-exchange resin is 4:1；
4. by step, 3. gained tritiated water to be measured measures with Low background liquid scintillation energy disperse spectroscopy the activity of tritium in tritiated water, according to tritium
The activity meter for changing tritium in water calculates the specific activity of tritiated water vapour in air.
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| CN106525494A (en) * | 2016-11-30 | 2017-03-22 | 上海新漫传感技术研究发展有限公司 | Sample replacing device for air tritiated water sampling device |
| CN108168955A (en) * | 2018-03-21 | 2018-06-15 | 阳江核电有限公司 | The accumulation sampling system and method for tritiated vapor in a kind of air |
| CN109444944B (en) * | 2018-12-21 | 2024-05-28 | 清华大学 | Method and device for rapidly and automatically analyzing tritium in water |
| CN110780332B (en) * | 2019-11-08 | 2021-06-29 | 中国原子能科学研究院 | System and method for measuring transformation rate of element state T and oxidation state T in environment |
| CN113270215B (en) * | 2021-05-18 | 2022-12-09 | 清华大学 | Liquid effluents from nuclear power plants 14 C automatic pretreatment device and treatment method |
| CN113654841A (en) * | 2021-09-18 | 2021-11-16 | 中国工程物理研究院核物理与化学研究所 | Device for quickly sampling tritiated water in air and method for measuring concentration of tritium in air |
| CN114210375B (en) * | 2021-10-23 | 2024-04-12 | 苏州思萃同位素技术研究所有限公司 | Preparation method of hydrogen isotope substituted acid |
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| CN103048163A (en) * | 2012-12-27 | 2013-04-17 | 核工业北京地质研究院 | Method for continuously extracting tritium from soil |
| CN103063482B (en) * | 2013-01-08 | 2015-04-15 | 中国工程物理研究院核物理与化学研究所 | Tritium-containing exhaust gas discharge monitoring automatic sampling system |
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